KR20200036890A - Pentachlorodisilane and method for producing purified reaction product comprising same - Google Patents

Abstract

A method for producing pentachlorodisilane is disclosed. The method includes partially reducing hexachlorodisilane with a metal hydride compound to provide a reaction product comprising pentachlorodisilane. The method further comprises purifying the reaction product to provide a purified reaction product comprising pentachlorodisilane. Purification reaction products comprising pentachlorodisilane formed according to the above method are also disclosed.

Description

Pentachlorodisilane and method for producing purified reaction product comprising same

Cross reference to related applications

This application claims priority and all interests to U.S. Provisional Application No. 62 / 538,858 filed on July 31, 2017, the contents of which are incorporated herein by reference.

Technology field

The present invention generally relates to a method for producing pentachlorodisilane, and more particularly, to a method for producing a purified reaction product containing pentachlorodisilane with excellent yield and conversion rate and a purified reaction product formed thereby. .

Silane compounds are known in the art and utilized for a variety of end use applications. For example, silane compounds can be used to prepare organopolysiloxanes, such as silicone polymers or resins. Alternatively, silane compounds are used very widely in the electronics industry. For example, silane compounds are used to form thin films through vapor deposition (eg, chemical vapor deposition, atomic layer deposition, etc.). The thin film may include crystalline silicon or silica (SiO ₂ ) depending on the choice of the silane compound used. Generally, these silane compounds include silicon-bonded hydrogen atoms (silicon hydride) and / or silicon-bonded halogen atoms.

One such example of a silane compound is pentachlorodisilane. However, pentachlorodisilane is difficult to synthesize and expensive to obtain otherwise. For example, one technique for synthesizing pentachlorodisilane involves oligomerizing a monosilane (eg, SiCl ₄ ) in the presence of hydrogen (H ₂ ). Another technique involves cleaving a silicon-silicon bond in a higher order silane compound (eg, tertiary or higher silane compound). However, this technique requires significant energy and / or expensive starting reagents.

The present invention provides a method for producing pentachlorodisilane. The method includes partially reducing hexachlorodisilane with a metal hydride compound to provide a reaction product comprising pentachlorodisilane. The method further comprises purifying the reaction product to provide a purified reaction product comprising pentachlorodisilane.

Also provided is a purification reaction product comprising pentachlorodisilane formed according to the method.

A method for producing pentachlorodisilane is disclosed. Pentachlorodisilane is produced as a purification reaction product and can be utilized for various end use applications. For example, pentachlorodisilane can be used as a starting component when preparing organopolysiloxanes, for example through co-hydrolysis and copolymerization. Alternatively or additionally, pentachlorodisilane can be used, for example, for the deposition of silicon (including polysilicon or monosilicon) or silica films.

The method includes partially reducing hexachlorodisilane with a metal hydride compound to provide a reaction product comprising pentachlorodisilane. The step of partially reducing the hexachlorodisilane with the metal hydride compound generally includes the step of combining the hexachlorodisilane and the metal hydride compound. The step of combining the hexachlorodisilane and the metal hydride compound may also be referred to as the step of contacting the hexachlorodisilane and the metal hydride compound. In other words, there is no preliminary step required for partial reduction other than the step of combining the hexachlorodisilane and the metal hydride compound.

“Partial reduction” means that hexachlorodisilane is partially reduced by a metal hydride compound to provide pentachlorodisilane compared to complete reduction of hexachlorodisilane with disilane. More specifically, partial reduction means that only one of the six silicon-bonded chlorine atoms is replaced or replaced with a silicon-bonded hydrogen atom to reduce the parent disilane (ie, hexachlorodisilane) once to provide pentachlorodisilane. . Partial reduction in the process of the present invention is limited to only one of the six silicon-bonded chlorine atoms providing pentachlorodisilane. Any of the six silicon-bonded chlorine atoms can be replaced with silicon-bonded hydrogen through the method of the present invention. For example, pentachlorodisilane may be represented by HCl ₂ Si * SiCl ₃ and / or Cl ₃ Si * SiCl ₂ H. As described below, partial reduction of hexachlorodisilane can produce byproducts other than pentachlorodisilane in the reaction product. For example, the reaction product may also include tetrachlorodisilane, trichlorodisilane, and the like. Also, as described below, the reaction product is purified in the process of the present invention to minimize and / or remove these byproducts from the reaction product, thereby providing a purified reaction product comprising pentachlorodisilane.

The present invention has technical and non-technical advantages. One of the problems solved by this process is to provide an improved pentachlorodisilane manufacturing process over conventional processes. For example, the method of the present invention generally produces pentachlorodisilane with higher purity, higher yield, greater selectivity, or a combination of any two or more of these than conventional processes. In addition, the method of the present invention can be scaled up for mass production of pentachlorodisilane, especially at lower cost than conventional processes.

As understood in the art, hexachlorodisilane has the formula Cl ₃ SiSiCl ₃ . The hexachlorodisilane can be synthesized, prepared or otherwise obtained. For example, hexachlorodisilane can be synthesized through chlorination of calcium silicide (CaSi ₂ ). Hexachlorodisilane is also commercially available from many suppliers.

The metal hydride compound may include any metal hydride compound capable of partially reducing hexachlorodisilane to provide pentachlorodisilane. Metal hydride compounds suitable for the purposes of the present invention are hydrides of sodium, magnesium, potassium, lithium, boron, calcium, titanium, zirconium, and aluminum, metal hydride compounds comprising at least one of these metals, and any of these Combinations of, but are not limited to. The metal hydride compound may be a simple (two-way) metal hydride compound or a complex metal hydride compound. The metal hydride compound may also contain elements, atoms, or substituents other than metal and hydrogen. For example, the metal hydride compound may include a substituted or unsubstituted hydrocarbyl group, hetero element, and the like.

In certain embodiments, the metal hydride compound is diisobutylaluminum hydride (DIBAH), dimethylaluminum hydride, diethylaluminum hydride, di (n-propyl) aluminum hydride, diisopropylaluminum hydride, di ( n-butyl) aluminum hydride, di (sec-butyl) aluminum hydride, di (tert-butyl) aluminum hydride, di (n-pentyl) aluminum hydride, di (iso-pentyl) aluminum hydride, di ( sec-pentyl) aluminum hydride, di (3-pentyl) aluminum hydride, di (tert-pentyl) aluminum hydride, di (neo-pentyl) aluminum hydride, isomer of dihexylaluminum hydride, diheptylaluminum hydride Isomers of Ride, Isomers of Dioctyl Aluminum Hydride, Isomers of Dinonyl Aluminum Hydride, Didecyl Aluminum Hydride Isomers, alkylaluminum dihydride, sodium bis (2-methoxyethoxy) aluminum hydride (eg, Vitride, Red-Al, etc.), aluminum hydride, lithium hydride, sodium hydride, sodium borohydride , Containing lithium aluminum hydride (e.g., LiAl (OtBu) ₃ H or LiAl (iBu) ₂ (OtBu) H, wherein tBu is tert-butyl and iBu is isobutyl), sodium aluminum hydride , Lithium borohydride, magnesium hydride, magnesium borohydride, calcium hydride, titanium hydride, zirconium hydride, tetramethylammonium borohydride, potassium borohydride and the like. Combinations of different metal hydride compounds, or combinations of metal hydride compounds and trialkylaluminum compounds can be used together. Any alkyl group can be independently selected from, for example, methyl, ethyl and isomer propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl and / or decyl.

In a specific embodiment, the metal hydride compound comprises diisobutylaluminum hydride (DIBAH), alternatively consisting essentially of, and alternatively consisting of.

In certain embodiments, the metal hydride compound is placed in a carrier vehicle such as a solvent or dispersant. If a carrier vehicle is present, it may include an organic solvent. Organic solvents include aromatic hydrocarbons, such as benzene, toluene, or xylene; Aliphatic hydrocarbons, such as heptane, hexane, or octane; Glycol ethers, such as propylene glycol methyl ether, dipropylene glycol methyl ether, propylene glycol n-butyl ether, propylene glycol n-propyl ether, or ethylene glycol n-butyl ether; Halogenated hydrocarbons such as dichloromethane, 1,1,1-trichloroethane, or methylene chloride; chloroform; Dimethyl sulfoxide; Dimethyl formamide; Acetonitrile; Tetrahydrofuran; White spirit; Mineral spirits; naphtha; n-methyl pyrrolidone; Or a combination thereof.

When placed in a carrier vehicle, the metal hydride compound generally provides 1 to 99, alternatively 10 to 80, alternatively 40 to 60% by weight, based on the combined weight of the metal hydride compound and carrier vehicle. It is present in the carrier vehicle in positive amounts.

Methods of making metal hydride compounds are well known in the art, and many of these compounds are commercially available from various suppliers.

The relative amount of metal hydride compound used may vary depending on the specific metal hydride compound selected, the reduction parameters used, and the like. The molar ratio of metal hydride compound to hexachlorodisilane used for partial reduction affects the conversion rate and / or conversion amount to pentachlorodisilane, and / or selectivity to pentachlorodisilane (i.e., by-product). Insane. Thus, the relative amounts of the metal hydride compound and hexachlorodisilane, as well as their molar ratios, can change. Generally, these relative amounts and molar ratios are selected to maximize the conversion and / or selectivity of partial reduction from hexachlorodisilane to pentachlorodisilane. For example, if a significant molar excess of metal hydride compound is used relative to hexachlorodisilane, by-products other than pentachlorodisilane of hexachlorodisilane (e.g., tetrachlorodisilane, trichlorodisilane, dichlorodi Excessive reduction to silane, etc.), formation of other by-products, and / or decomposition of hexachlorodisilane, pentachlorodisilane, and the like may occur.

In certain embodiments, the molar ratio of hexachlorodisilane to metal hydride compound is 1: 0.01 to 1: 3, alternatively 1: 0.05 to 1: 1.25, alternatively 1: 0.1 to 1: 1.2, alternatively 1: 0.2 to 1: 1.1, alternatively 1: 0.3 to 1: 1, alternatively 1: 0.4 to 1: 0.9, alternatively 1: 0.5 to 1: 0.8.

Generally, partial reduction of hexachlorodisilane to produce a reaction product comprising pentachlorodisilane is performed in a vessel or reactor. The hexachlorodisilane and metal hydride compound may be supplied to the container together or separately, or may be placed in the container in any order of addition. When the partial reduction is performed at a high temperature, the vessel or reactor can be heated in any suitable manner, for example through a jacket, as described below.

The hexachlorodisilane and metal hydride compound may be supplied to the container sequentially or at a time over a period of time.

Parameters can be modified during partial reduction of hexachlorodisilane to prepare a reaction product comprising pentachlorodisilane. For example, temperature, pressure, and other parameters can be independently selected or modified during partial reduction of hexachlorodisilane to prepare a reaction product comprising pentachlorodisilane. Any of these parameters are independently ambient (e.g., room temperature and / or atmospheric pressure) and / or non-ambient parameters (e.g., low or high temperature and / or reduced pressure or high pressure). Can be Any parameter may also be a dynamic parameter that is modified in real time, ie during the method of the present invention, or it can be a static parameter.

In certain embodiments, partial reduction of hexachlorodisilane to prepare a reaction product comprising pentachlorodisilane is performed at high temperature.

The high temperature is generally above room temperature (eg, 22-25 ° C) to 150 ° C, alternatively 30 to 140 ° C, alternatively 40 to 130 ° C, alternatively 50 to 120 ° C, alternatively 60 to 110 ° C, alternatively 70 to 100 ° C, alternatively 75 to 95 ° C, alternatively 80 to 90 ° C.

The hexachlorodisilane and / or metal hydride compound can be independently heated and blended, blended and heated (before, during, and / or after such blending) and the like. In certain embodiments, hexachlorodisilane is heated to a high temperature, and the metal hydride compound is combined with hexachlorodisilane at a high temperature. The hexachlorodisilane and the metal hydride compound may be blended simultaneously, gradually blended, or in other ways. The metal hydride compound may be gradually blended with hexachlorodisilane over a period of time.

The hexachlorodisilane and the metal hydride compound can be stored independently, under anhydrous (ie, without water) conditions, an inert atmosphere, or generally both, ie, anhydrous inert atmosphere. The inert atmosphere is generally a gas containing molecular nitrogen, helium, argon, or a mixture of any two or more of them. Similarly, partial reduction of hexachlorodisilane to prepare a reaction product comprising pentachlorodisilane can be performed under anhydrous conditions and / or inert atmosphere.

The method may further include the step of stirring the hexachlorodisilane and the metal hydride compound. Stirring can enhance their mixing and mutual contact when hexachlorodisilane and metal hydride compounds are blended (including stirring in their reaction mixtures). This contact can use other conditions independently, under stirring (eg, simultaneously or sequentially), or without stirring (ie, irrespective of stirring, alternatively instead of stirring). Other conditions can be adjusted to enhance the contact of hexachlorodisilane and thus the reaction (ie, partial reduction) to form pentachlorodisilane in a specific contact step. Other conditions may be consequently effective conditions to improve the reaction yield or to minimize the amount of specific reaction by-products included in the reaction product with pentachlorodisilane.

The time required for partial reduction of hexachlorodisilane to prepare a reaction product containing pentachlorodisilane is a function of scale, reaction parameters and conditions, selection of metal hydride compounds, and the like. In a specific embodiment, the time required for partial reduction of hexachlorodisilane to prepare a reaction product comprising pentachlorodisilane is greater than 0 to 24 hours after combining the hexachlorodisilane and the metal hydride compound, Alternatively greater than 0 to 12 hours, alternatively greater than 0 to 6 hours, alternatively greater than 0 to 2 hours.

In certain embodiments, partial reduction of hexachlorodisilane to prepare a reaction product comprising pentachlorodisilane is performed without a carrier vehicle or solvent. For example, no carrier vehicle or solvent may be formulated separately from hexachlorodisilane and / or metal hydride compounds. In these or other embodiments, the hexachlorodisilane and the metal hydride compound are also placed in the carrier vehicle or solvent such that there is no carrier vehicle or solvent during partial reduction due to the hexachlorodisilane and / or metal hydride compound. Does not work.

Alternatively, partial reduction can be performed in the presence of a carrier vehicle or solvent. Specific examples of these are mentioned above in relation to potential carrier vehicles for metal hydride compounds.

As mentioned above, the reaction product can include various by-products resulting from partial reduction of hexachlorodisilane. These are other reduced forms of hexachlorodisilane, such as tetrachlorodisilane, trichlorodisilane, dichlorodisilane, etc., residual and / or unreacted amounts of hexachlorodisilane and / or metal hydride compounds, or their Decomposition products. The reaction products also generally include metal chlorides formed from metal hydride compounds upon partial reduction of hexachlorodisilane. The metal chloride present in the reaction product is generally a function of the metal hydride compound used. For example, when the metal hydride compound includes diisobutylaluminum hydride, the metal chloride compound may include diisobutylaluminum chloride. If partial reduction of hexachlorodisilane is performed in any carrier vehicle or solvent, the reaction product generally also includes such carrier vehicle or solvent. However, this method is generally carried out purely, ie without solvent, so this is not the usual case. Metal chlorides are generally liquid in the reaction products.

The method further comprises purifying the reaction product to provide a purified reaction product comprising pentachlorodisilane. Any suitable purification technique can be used. Examples of suitable techniques include distillation, evaporation, extraction, freeze drying, gas chromatography, ion exchange chromatography, reverse phase liquid chromatography, stripping, and / or volatilization.

In certain embodiments, purifying the reaction product comprises distilling the reaction product to provide a purification reaction product. In a specific embodiment, distilling the reaction product produces a crude reaction product comprising pentachlorodisilane, and the method further comprises purifying the crude reaction product to provide a purified reaction product.

For example, the reaction product can be distilled upon formation so that the crude reaction product is condensed and recovered. The crude reaction product has a higher content of pentachlorodisilane than the reaction product. In certain embodiments, the crude reaction product is 5 to 70, alternatively 6 to 47, alternatively 7 to 44, alternatively 8 to 41, alternatively 9 to based on the total weight of the crude reaction product. Pentaclo in an amount of 38, alternatively 10 to 35, alternatively 11 to 32, alternatively 12 to 29, alternatively 13 to 26, alternatively 14 to 23, alternatively 15 to 20% by weight Rhodisilane. The concentration of pentachlorodisilane in the crude reaction product may differ from the range presented herein. The concentration of pentachlorodisilane in the crude reaction product can be measured by known methods, such as gas chromatography, optionally via gas chromatography-thermal conductivity detector.

Distillation of the reaction product to produce a crude reaction product comprising pentachlorodisilane is generally performed at (i) high temperature, (ii) reduced pressure, or (iii) high temperature and reduced pressure. High or low means that compared to room temperature and atmospheric pressure. As understood in the art, the number of trays used for distillation can be optimized and can affect the concentration or yield of pentachlorodisilane. For example, the use of a larger number of trays via distillation can increase the concentration or yield of pentachlorodisilane in the crude reaction product.

The high temperature is generally above room temperature to 150 ° C, alternatively 30 to 140 ° C, alternatively 40 to 130 ° C, alternatively 50 to 120 ° C, alternatively 60 to 110 ° C, alternatively 70 to 100 ° C , Alternatively 75 to 95 ° C, alternatively 80 to 90 ° C. Any pressure reduction between vacuum and atmospheric pressure can be used, but pressure reduction is generally operated as a vacuum. For example, the reduced pressure is greater than 0 to 200, alternatively greater than 0 to 100, alternatively greater than 0 to 90, alternatively greater than 0 to 80, alternatively greater than 0 to 70, alternatively greater than 0 to 60 , Alternatively greater than 0 to 50, alternatively greater than 0 to 40, alternatively greater than 0 to 30, alternatively greater than 0 to 20, alternatively 5 to 15 Torr. For example, if the reaction product comprises any carrier vehicle or solvent, the high temperature may differ from the ranges given above.

The crude reaction product can be condensed and recovered at any suitable temperature. In certain embodiments, the crude reaction product condenses at a temperature of 0 to 25 ° C, alternatively 0 to 20 ° C, alternatively 0 to 15 ° C, alternatively 0 to 10 ° C, alternatively 4 to 6 ° C do.

If the method further comprises the step of purifying the crude reaction product to provide a purified reaction product, the crude reaction product can be purified through any suitable technique. The purification technology may be the same or different from the purification technology used to prepare the crude reaction product from the reaction product. In certain embodiments, purifying the crude reaction product to provide a purified reaction product includes distilling the crude reaction product. In a specific embodiment, the step of purifying the crude reaction product includes fractional distillation of the crude reaction product. The following description regarding the parameters for the purification of the crude reaction product applies whether distillation is used or fractional distillation is used.

As with the distillation of the reaction product, the distillation of the crude reaction product is generally carried out at (i) high temperature, (ii) reduced pressure, or (iii) high temperature and reduced pressure. High or low means that compared to room temperature and atmospheric pressure. As mentioned above and as understood in the art, the number of trays used for distillation can be optimized and can affect the concentration or yield of pentachlorodisilane. For example, using a larger number of trays via distillation can increase the concentration or yield of pentachlorodisilane.

The high temperature is generally above room temperature to 150 ° C, alternatively 30 to 140 ° C, alternatively 40 to 130 ° C, alternatively 50 to 120 ° C, alternatively 60 to 110 ° C, alternatively 70 to 100 ° C , Alternatively 75 to 95 ° C, alternatively 80 to 90 ° C. Any pressure reduction between vacuum and atmospheric pressure can be used, but pressure reduction is generally operated as a vacuum. For example, the reduced pressure is greater than 0 to 200, alternatively greater than 0 to 100, alternatively greater than 0 to 90, alternatively greater than 0 to 80, alternatively greater than 0 to 70, alternatively greater than 0 to 60 , Alternatively greater than 0 to 50, alternatively greater than 0 to 40, alternatively greater than 0 to 30, alternatively greater than 0 to 20, alternatively 5 to 15 Torr.

In certain embodiments, distillation of the crude reaction product uses more trays or plates than distillation of the reaction product. However, as understood in the art, the number of trays or plates can be changed, and the feeding position can be optimized or changed.

In general, distillation of the crude reaction product involves multiple purification steps. For example, distillation and / or fractional distillation can be repeated any number of times to further concentrate pentachlorodisilane in the purification reaction product. Purification reaction product refers to the final form of the composition resulting from any number of purification steps applied to the reaction product.

For example, distillation of the crude reaction product can produce a first concentrated reaction product. Distillation of the first concentrated reaction product can then produce a second concentrated reaction product. Distillation of the second concentrated reaction product can then produce a third concentrated reaction product. Due to the relative concentration of pentachlorodisilane in the concentrated reaction product compared to other components in the particular concentrated reaction product (e.g., by-products, starting materials, etc.), each iteration of the reaction product is distinct from the previous iteration (i.e. , The third concentrated reaction product is distinguished from the second concentrated reaction product, and the second concentrated reaction product is distinguished from the first concentrated reaction product). Specifically, the relative concentration (ie, purity) of pentachlorodisilane increases through each repeat purification step. Each repeat purification step can be selected independently.

Thus, to increase the concentration of pentachlorodisilane in the purification reaction product, purification of the crude reaction product generally produces a first concentrated reaction product, followed by further purification of the first concentrated reaction product. In certain embodiments, the first concentrated reaction product is 20 to 83, alternatively 22 to 80, alternatively 24 to 77, alternatively 26 to 74, alternatively, based on the total weight of the first concentrated reaction product. 28 to 71, alternatively 30 to 68, alternatively 32 to 65, alternatively 34 to 62, alternatively 36 to 59, alternatively 38 to 56, alternatively 40 to 53, alternatively 42 Pentachlorodisilane in an amount of to 50% by weight. The concentration of pentachlorodisilane in the first concentrated reaction product may differ from the range presented herein. For example, distillation of the crude reaction product can include additional trays or plates that can be used to provide additional purification in a single purification step.

The concentration of pentachlorodisilane in the first concentrated reaction product can be measured by known methods, such as gas chromatography, optionally through a gas chromatography-thermal conductivity detector.

Each repeat purification step can be independently selected, but in certain embodiments, each repeat purification step includes distillation. Even in this embodiment, parameters related to distillation (eg, high temperature and / or reduced pressure) can be independently selected through each repeated distillation step. However, in general, each repeated distillation step uses the parameters specified above for high temperature and reduced pressure.

In certain embodiments, the method provides at least one, alternatively at least two, alternative to preparing a crude reaction product comprising pentachlorodisilane to provide a purified reaction product comprising pentachlorodisilane It typically includes three repeat distillation steps. However, the method is not limited to this, and any number of repeated distillation steps or repeated purification steps may be used. The number of repeat distillation steps, or repeat purification steps, generally depends on the desired concentration of pentachlorodisilane in the purification reaction product.

Any number of individual reaction products, crude reaction products, or concentrated reaction products can be combined to form a batch. In certain embodiments, multiple crude reaction products prepared independently are combined to form a batch of crude reaction products. The batch of crude reaction product is then purified according to this method to provide pentachlorodisilane.

In certain embodiments, the purification reaction product is at least 50, alternatively at least 55, alternatively at least 60, alternatively at least 65, alternatively at least 70, alternatively at least 75 based on the total weight of the purification reaction product. , Alternatively at least 80, alternatively at least 81, alternatively at least 82, alternatively at least 83, alternatively at least 84, alternatively at least 85, alternatively at least 86, alternatively at least 87, alternatively Alternatively at least 88, alternatively at least 89, alternatively at least 90, alternatively at least 91, alternatively at least 92, alternatively at least 93, alternatively at least 94, alternatively at least 95, alternatively Pentachlorodisilane in an amount of at least 96, alternatively at least 97, alternatively at least 97.5, alternatively at least 98 wt%. According to several repeated purification steps, the concentration of pentachlorodisilane in the purification reaction product is 100, alternatively 99.9999999, alternatively 99.999999, alternatively 99.99999, alternatively 99.9999, alternatively 99.999, alternatively 99.99, Alternatively 99.9, alternatively 99.0 wt%.

In addition to the reaction products, crude reaction products, and / or by-products that may be present in the purification reaction products, various trace metals may also be present in any of these reaction products, including purification reaction products. These trace metals can be attributed to the metal hydride compounds used or other sources (e.g. trace metals resulting from the production of hexachlorodisilane (e.g., prepared through a direct process)). For example, in certain embodiments, the purification reaction product comprises aluminum in an amount of less than 50 ppb.

It is to be understood that the appended claims are not limited to the expressions and specific compounds, compositions, or methods described in the specific content for carrying out the invention, and they may vary depending on the specific embodiments falling within the scope of the appended claims. With respect to any Markush group used herein to describe specific features or aspects of various embodiments, it is different from, and / or distinct from, each member of each Markush group independently of all other Markush members. , You may get unexpected results. Each member of the Markush group may be used individually and / or in combination, and appropriately supports a particular embodiment within the scope of the appended claims.

In addition, all ranges and subranges used to describe various embodiments of the present invention, independently and collectively, are within the scope of the appended claims, and the full and / or partial values (such values herein. It is understood that all ranges are inclusive and contemplated even if not specified in the above. Those skilled in the art readily recognize that the listed ranges and sub-ranges fully represent and enable various embodiments of the present invention, such ranges and sub-ranges being suitable 1/2, 1/3, 1/4, 1/5, etc. It can be expressed in more detail. As an example, the range of “0.1 to 0.9” can be more specifically expressed as the lower 1/3, ie 0.1 to 0.3, the middle 1/3, ie 0.4 to 0.6, and the upper 1/3, ie 0.7 to 0.9. And, individually and collectively, are within the scope of the appended claims, and may be used individually and / or collectively and appropriately support certain embodiments within the scope of the appended claims. Further, with respect to expressions defining or modifying a range of "above", "excess", "below", "below", it should be understood that such expressions include subranges and / or upper or lower limits. As another example, a range of “at least 10” essentially includes at least 10 to 35 subranges, at least 10 to 25 subranges, 25 to 35 subranges, and the like, each subrange individually and / or Or it can be used collectively and appropriately supports a particular embodiment within the scope of the appended claims. Finally, individual numbers within the disclosed ranges may be used, which appropriately support certain embodiments within the scope of the appended claims. For example, a range of “1 to 9” includes several individual integers (eg 3) as well as individual numbers (eg 4.1) including decimal points (or fractions), which are used within the scope of the appended claims. Specific embodiments can be adequately supported.

The following examples are intended to illustrate the invention and should not be regarded as limiting the scope of the invention in any way.

Example

Example 1: Preparation of pentachlorodisilane

Partial reduction of hexachlorodisilane : Hexachlorodisilane (3.48 kg; 12.9 mol) is placed in a 12 L jacketed reactor and heated and maintained at a temperature of 80 ° C. Subsequently, the contents of the reactor were maintained at a temperature of 80 to 90 ° C., and a metal hydride compound (DIBAH; 1.48 kg; 10.4 mol) was added over 2 hours while stirring to obtain a reaction mixture. The reaction mixture was stirred in the reactor for 30 minutes, then distilled through a 5-tray column under vacuum to obtain a reaction product comprising pentachlorodisilane (PCDS) (about 3.2 kg; 16 via GC-TCD integration). % PCDS), which is then condensed through a cooled condenser (5 ° C.) and recovered in a 3 L recovery flask. Subsequently, the reaction product was fractionally distilled under vacuum (decompression to 10 Torr) at a port temperature of 80 ° C. through a 20-tray column to obtain a crude reaction product comprising pentachlorodisilane (PCDS) (494 g; PCDS of 46% via GC-TCD integration).

Purification of the crude reaction product containing pentachlorodisilane: After partial reduction of hexachlorodisilane and subsequent distillation are repeated 18 times, the resulting crude reaction products are combined with each other to combine the crude with pentachlorodisilane. The reaction product is obtained (13.6 kg). Subsequently, the combined crude reaction product was fractionally distilled three times under vacuum (decompression to 10 Torr) at a pot temperature of 80 ° C. to obtain a purification reaction product containing pentachlorodisilane (PCDS) (2.8 kg; GC- 98 +% PCDS via TCD). The purified reaction product was then analyzed for 23 metals by ICP-MS with a detection limit of 10 ppb to give a total trace metal content of 89 ppb, including 10 ppb Al.

The invention has been described by way of example, and the terms used should be understood to be illustrative and not restrictive. Obviously, many modifications and variations of the invention are possible in light of the above teachings. The invention may be practiced differently than specifically described.

Claims (14)

As a method for producing pentachlorodisilane,
Partially reducing hexachlorodisilane with a metal hydride compound to provide a reaction product comprising pentachlorodisilane; And
A method comprising purifying the reaction product to provide a purified reaction product comprising pentachlorodisilane. The method of claim 1, wherein the metal hydride compound comprises diisobutylaluminum hydride (DIBAH). The method of claim 1 or 2, wherein the purification reaction product comprises pentachlorodisilane in an amount of at least 95 wt% based on the total weight of the purification reaction product. The method of claim 3, wherein the purification reaction product comprises pentachlorodisilane in an amount of at least 98 wt% based on the total weight of the purification reaction product. The method according to any one of claims 1 to 4, wherein purifying the reaction product comprises distilling the reaction product to provide a purified reaction product. 6. The method of claim 5, wherein distilling the reaction product produces a crude reaction product comprising pentachlorodisilane, the method further comprising purifying the crude reaction product to provide a purified reaction product. , Way. The method of claim 6, wherein purifying the crude reaction product comprises fractional distillation of the crude reaction product to provide a purified reaction product. The method according to any one of claims 5 to 7, wherein distilling the reaction product is carried out at reduced pressure and high temperature. 9. The method of claim 8, wherein (i) the reduced pressure is greater than 0 to 50 Torr; (ii) the high temperature is 70 to 90 ° C; Or (iii) both (i) and (ii). The method according to any one of claims 1 to 9, wherein (i) the hexachlorodisilane and the metal hydride compound are used in a molar ratio of 1: 0.01 to 1: 3; (ii) the method is carried out without solvent; (iii) the step of partially reducing hexachlorodisilane is carried out at high temperature; (iv) purifying the reaction product comprises a plurality of purification steps; Or (v) any combination of (i) to (iv). A purification reaction product comprising pentachlorodisilane, formed according to the method of claim 1. 12. The purification reaction product of claim 11 comprising pentachlorodisilane in an amount of at least 95 wt% based on the total weight of the purification reaction product. 12. The purification reaction product of claim 11 comprising pentachlorodisilane in an amount of at least 98 wt% based on the total weight of the purification reaction product. The purification reaction product according to any one of claims 11 to 13 comprising aluminum in an amount of less than 50 ppb.